反应详情

温度

0 °C

To a solution of 5-methoxy-2-nitrobenzoic acid (18.0 g, 91.3 mmol) and DMF (0.1 mL) in THF (150 mL) was added dropwise oxalyl chloride (12.7 g, 100 mmol) under ice-cooling, and the mixture was stirred at 0° C. for 1 hr, and then at room temperature for 3 hr. This solution was added dropwise to aqueous ammonia (7% aqueous solution, 200 mL) under ice-cooling. The reaction solution was concentrated under reduced pressure to evaporated THF, and the precipitated insoluble material was collected by filtration. The filtered cake was washed with water to give 5-methoxy-2-nitrobenzamide as a pale-yellow powder (10.0 g, 56%).

1. temperaturecooling
2. waitat room temperature for 3 hr
3. temperaturecooling
4. concentrationThe reaction solution was concentrated under reduced pressure
5. customto evaporated THF
6. filtrationthe precipitated insoluble material was collected by filtration
7. washThe filtered cake was washed with water